CN105367922B - 环保节能自然交联橡胶材料及其生产方法 - Google Patents
环保节能自然交联橡胶材料及其生产方法 Download PDFInfo
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- CN105367922B CN105367922B CN201510983116.6A CN201510983116A CN105367922B CN 105367922 B CN105367922 B CN 105367922B CN 201510983116 A CN201510983116 A CN 201510983116A CN 105367922 B CN105367922 B CN 105367922B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
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- H—ELECTRICITY
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- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
本发提供一种环保节能自然交联橡胶材料及其生产方法,是将橡胶、聚烯烃、相容剂、硅烷偶联剂、引发剂、催化剂、促进剂、活性剂、防老剂、抗氧剂、软化剂、润滑剂、阻燃剂、补强剂、填充剂在捏炼机混炼10～12分钟，混炼好的材料由温度为40～90℃虑橡机过滤，在辗页机上辗成厚度0.7‑2mm的橡胶薄片经过冷却，而制得环保节能自然交联橡胶材料。它具有节能和环保双重特性，采用环保节能自然交联橡胶材料挤出橡胶电缆不需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，减少了生产工艺过程，不需要硫化设备，明显降低了投资成本和生产成本，显著降低了二氧化碳的排放量和能源消耗。
Description
技术领域：
本发明涉及环保节能自然交联橡胶材料及其生产方法, 橡胶材料不含对人体和环境有重大危害的铅（Pb）、镉（Cd）、汞（Hg）、六价铬（Cr）重金属、多溴联苯及其醚类等有悖于环保要求的物质，采用环保节能自然交联橡胶材料挤出橡胶电缆不需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，在空气中放置一周左右时间即可自然实现交联，减少了生产工艺过程，不需要硫化设备，明显降低了投资成本和生产成本，显著降低了二氧化碳的排放量和能源消耗。
背景技术：
现在使用的橡胶绝缘电缆挤出后需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，需要对硫化设备进行大量的投资，消耗大量的能源，并且排放大量的二氧化碳，生产成本较高。环保节能自然交联橡胶材料挤出橡胶电缆后电缆在空气中放置一周左右时间即可自然实现交联，不需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，减少了生产工艺过程，不需要硫化设备，明显降低了投资成本和生产成本，同时显著降低了能源消耗和二氧化碳的排放量。
环保节能自然交联橡胶材料，不含对人体和环境有重大危害的铅（Pb）、镉（Cd）、汞（Hg）、六价铬（Cr）重金属、多溴联苯及其醚类等有悖于环保要求的物质，是很好的环保节能橡胶材料。随着我国国民经济的发展，我国的橡胶材料需求快速增长，特别是环保节能自然交联橡胶材料需求量比较大。环保节能自然交联橡胶材料符合节能和绿色环保设计与制造的要求。
因此期望开发出具有优良环保、节能性能的自然交联橡胶材料，但迄今为止尚未有这样的具有优异环保及节能性能的自然交联橡胶材料公开报道。
发明内容：
综上所述，本发明的目的是针对目前使用的橡胶在电缆挤出后需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，需要对硫化设备进行大量的投资，消耗大量的能源，并且排放大量的二氧化碳，生产成本高的问题，而研制的一种环保节能自然交联橡胶材料及其生产方法，该环保节能自然橡胶材料不仅能够满足环保性能要求，而且使电线电缆生产过程不需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，不需要硫化设备，明显降低了投资成本和生产成本，同时显著降低了能源消耗和二氧化碳的排放量。
本发明的技术方案是通过以下方式实现的：
一种环保节能自然交联橡胶材料，是由以下重量原料制备而成：
组 成 配 比（重量份数）
橡胶 100
聚烯烃 15～30
相容剂 5～10
硅烷偶联剂 2～3.5
引发剂 0.1～0.3
催化剂 2～3.5
促进剂 1.5～3
活性剂 8～10
抗氧剂 1～1.5
防老剂 1～2
软化剂 5～10
润滑剂 1～2.5
阻燃剂 30～60
补强剂 30～50
填充剂 80～100
进一步，所述的橡胶为三元乙丙橡胶（EPDM）或丁基橡胶(IIR)或天然橡胶(NR)。
进一步，所述的聚烯烃为乙烯一醋酸乙烯共聚物(EVA)或乙烯一丙烯酸乙酯共聚物(EEA)或乙烯一甲基丙烯酸酯共聚物（EMA）或乙烯一丙烯酸丁酯共聚物（EBA）或乙烯一丙烯酸共聚物（EAA）或乙烯一甲基丙烯酸共聚物（EMAA）或乙烯一辛烯共聚物(POE)。
进一步，所述的相容剂为马来酸酐接枝EVA或马来酸酐接枝聚乙烯或马来酸酐接枝三元乙丙橡胶。
进一步，所述的硅烷偶联剂为乙烯基三甲基硅烷(A-171)或乙烯基三（β-甲基乙氧基）硅烷(A-172)或乙烯基三乙氧基硅烷(A-151)。
进一步，所述的引发剂为2,5一二甲基乙烷(DHBP)或过氧化二异丙苯(DCP)或叔丁基过氧化一3,5,5一三甲基己酸酯（TBPT）。
进一步，所述的催化剂为二月桂酸二丁基锡(DBTBL)或二丁基醋酸锡或二丁基马来酸锡。
进一步，所述的促进剂为N-环己基-2-苯并噻唑次磺酰胺(促进剂CZ)或二硫化四甲基秋兰母(促进剂TMTD)或二硫化四乙基秋兰母(促进剂TETD)或二硫化二苯并噻唑（促进剂DM）或四硫化双五次甲基秋兰母(促进剂DPTT)。
进一步，所述的活性剂为轻质MgO或轻质ZnO。
进一步，所述的抗氧剂为1076（β-（3,5-二叔丁基-4-羟基苯基）丙酸正十八碳醇酯）或264（2,6-二叔丁基对甲酚）或1010（四[β-(3,5-二叔丁基-4羟基苯基)丙酸]季戊四醇酯）或300（4,4'-硫代双(6-叔丁基-3-甲基苯酚)）。
进一步，所述的防老剂为RD（2,2,4-三甲基-1,2-二氢化喹啉聚合体）或防老剂4010(CPPD)（N-苯基-N’-环己基对苯二胺）或防老剂MB（2—硫醇基苯并咪唑）或防老剂DNP（N,N’-二（β-萘基）对苯二胺）或防老剂H（N,N’-二苯基对苯二胺）或防老剂D（N-苯基- β -萘胺）。
进一步，所述的软化剂为石蜡或硬脂酸丁酯或对苯二甲酸二辛酯或邻苯二甲酸二辛酯或邻苯二甲酸二丁酯或己二酸二辛酯或葵二酸二辛酯。
进一步，所述的润滑剂为乙撑二乙酰胺或硬脂酸或硬脂酸锌或硬脂酸钙。
进一步，所述的阻燃剂为硅氮聚合物或氢氧化铝或氢氧化镁。
进一步，所述的补强剂为白炭黑或高耐磨炭黑或半补强炭黑或漕法炭黑或炉法炭黑。
进一步，所述的填充剂为碳酸钙或滑石粉或陶土。
进一步，三元乙丙橡胶为白色颗粒、丁基橡胶(IIR) 为白色块状物、天然橡胶(NR)为浅黄色块状物。
进一步， 聚烯烃EVA、EEA、EMA、EBA、EAA、EMAA、POE为白色颗粒。
进一步，相容剂马来酸酐接枝EVA、马来酸酐接枝聚乙烯、马来酸酐接枝三元乙丙橡胶为白色颗粒。
进一步，硅烷偶联剂A-171、A-172、A-151为无色透明液体。
进一步，引发剂DHBP或TBPT为淡黄色透明液体，DCP为粉末状白色颗粒。
进一步，催化剂DBTBL、二丁基醋酸锡为无色透明液体，二丁基马来酸锡为粉末状无色颗粒。
进一步，促进剂CZ、DM为粉末状黄色颗粒，促进剂TMTD、TETD、DPTT为粉末状白色颗粒。
进一步，活性剂为轻质MgO、轻质ZnO为粉末状白色颗粒。
进一步，抗氧剂1076、264、1010、300为粉末状白色颗粒。
进一步，防老剂RD为粉末状琥珀色颗粒， 4010(CPPD)、MB为粉末状白色颗粒，DNP为粉末状灰色颗粒，H为粉末状灰褐色颗粒，RD为粉末状棕色颗粒。
进一步，软化剂为石蜡为白色颗粒，硬脂酸丁酯、对苯二甲酸二辛酯、邻苯二甲酸二辛酯、邻苯二甲酸二丁酯、己二酸二辛酯、葵二酸二辛酯为无色透明液体。
进一步，润滑剂为乙撑二乙酰胺、硬脂酸、硬脂酸锌、硬脂酸钙为粉末状白色颗粒。
进一步，阻燃剂硅氮聚合物、氢氧化铝、氢氧化镁为粉末状白色颗粒。
进一步，补强剂白炭黑为粉末状白色颗粒，高耐磨炭黑、半补强炭黑、漕法炭黑、炉法炭黑为粉末状黑色颗粒
进一步，填充剂碳酸钙、滑石粉、陶土为粉末状白色颗粒。
本发明的生产方法是：
一种环保节能自然交联橡胶材料的生产方法包括以下步骤，先将橡胶、聚烯烃、相容剂、硅烷偶联剂、引发剂、催化剂、促进剂、活性剂、防老剂、抗氧剂、软化剂、润滑剂、阻燃剂、补强剂、填充剂在捏炼机混炼10～12分钟；再将混炼好的材料由温度为40～90℃虑橡机过滤；将过滤后的橡胶材料在辗页机上辗成厚度0.7-2mm的橡胶薄片，经过冷却后制得环保节能自然交联橡胶材料。
本发明生产的环保节能自然交联橡胶材料由以下技术指标证明它无毒，无腐蚀、不污染环境。
其主要技术指标：
长期使用温度 90℃
拉伸强度 8.6MPa
断裂伸长率 467%
拉伸强度变化 率 8.5%
断裂伸长变化率 6.7%
载荷下伸长率 20%
冷却后永久变形率 5%
20℃时体积电阻率 2.9×1013 Ω•m
氧指数 28
烟密度（有焰） 77
卤酸气体含量 0 mg/g
电导率 7.6μs/mm
铅（Pb）含量 ≤5×10-6
镉（Cd）含量 ≤5×10-6
六价铬（Cr）含量 ≤5×10-6
汞（Hg）含量 ≤5×10-6
多溴联苯含量 ≤5×10-6
多溴联苯醚类含量 ≤5×10-6
本发明的积极效果是：
本发明制得的环保节能自然交联橡胶材料无毒，无腐蚀、不污染环境，具有以下优点：
1．环保节能自然交联橡胶材料是按照相关的环保要求，对添加剂进行严格的筛选，使配方体系中不含对人体和环境有很大危害的铅（Pb）、镉（Cd）、汞（Hg）、六价铬（Cr）重金属、多溴联苯及其醚类等有悖于环保要求的物质，不会对环境造成污染，因而使用起来更加放心、可靠，社会效益显著；
2．环保节能自然交联橡胶材料挤出橡胶电缆后电缆在空气中放置一周左右时间即可实现自然交联，不需要经过蒸汽硫化或辐照交联或硅烷交联水煮硫化，不需要硫化设备，减少了生产工艺，明显降低了投资成本和生产成本，同时显著降低了能源消耗和二氧化碳的排放量；而且橡胶材料符合国家发展节能环保经济的产业政策，经济效益显著；
3．该环保节能自然交联橡胶材料是很好的节能环保材料，使用上述环保节能自然交联橡胶材料，经橡胶电缆挤出机50～80℃挤出，可生产电力电缆、船用电缆、矿用电缆、通用橡套电缆等产品。环保节能自然交联橡胶材料符合节能和绿色环保设计与制造的要求。
具体实施方式：
下面结合实施例对本发明作进一步的详细说明。
实施例1. （以生产电力电缆材料为例）
一种环保节能自然交联橡胶材料，是由以下重量原料制备而成：
组 成 配 比（重量份数）
丁基橡胶(IIR) 100
乙烯一醋酸乙烯共聚物(EVA) 15
相容剂为马来酸酐接枝EVA 5
硅烷偶联剂A-172 2
引发剂DCP 0.1
催化剂DBTBL 2
促进剂TETD 1.5
活性剂氧化锌 10
抗氧剂264 1
防老剂MB 1
软化剂石蜡 10
润滑剂硬脂酸 1
氢氧化铝阻燃剂 60
补强剂为半补强炭黑 50
填充剂为碳酸钙 80
本发明的生产方法是按上述配比先将丁基橡胶(IIR)、乙烯一醋酸乙烯共聚物(EVA)、相容剂马来酸酐接枝EVA、硅烷偶联剂A-172、引发剂DCP、催化剂DBTBL、促进剂TETD、活性剂氧化锌、抗氧剂264、防老剂MB、软化剂石蜡、润滑剂硬脂酸、氢氧化铝阻燃剂、补强剂半补强炭黑和填充剂碳酸钙放到捏炼机混炼10～12分钟；再将混炼好的材料在温度为40～90℃虑橡机过滤；将过滤后的橡胶材料在辗页机上辗成厚度0.7-2mm的橡胶薄片，经过冷却后制得环保节能自然交联橡胶材料；生产的橡胶材料的拉伸强度为8.8MPa，断裂伸长率为467%；用电缆挤橡机在50～80℃挤出生产电力电缆、船用电缆、矿用电缆、通用橡套电缆等电缆产品。
使用本环保节能自然交联橡胶材料生产电力电缆的材料性能如下：
| 实验内容 | 实施例1 |
| 拉伸强度变化率 | 8.3% |
| 断裂伸长变化率 | 7.4% |
| 载荷下伸长率 | 20% |
| 冷却后永久变形 | 3% |
实施例2
实施例2和实施例1同样是以生产电力电缆材料为例， 其它的同实施例1，所不同的聚烯烃为乙烯一丙烯酸共聚物（EAA），促进剂为四硫化双五次甲基秋兰母（促进剂DPTT）。
实施例3
实施例3和实施例1同样是以生产电力电缆材料为例，其它的同实施例1，所不同的是聚烯烃为乙烯一甲基丙烯酸酯共聚物（EMA），润滑剂为乙撑二乙酰胺。
实施例4（以生产矿用电缆材料为例）
一种环保节能自然交联橡胶材料，是由以下重量原料制备而成：
组 成 配 比（重量份数）
三元乙丙橡胶（EPDM） 100
乙烯一丙烯酸乙酯共聚物(EEA) 30
相容剂为马来酸酐接枝PE 10
硅烷偶联剂A-171 3.5
引发剂DHBP 0.3
催化剂二丁基醋酸锡 3.5
促进剂DM 3
活性剂氧化镁 8
抗氧剂1010 1.5
防老剂RD 2
软化剂邻苯二甲酸二辛酯 5
润滑剂硬脂酸钙 2.5
硅氮聚合物 30
补强剂为白炭黑 30
填充剂为陶土 100
本发明的生产方法是按上述配比先将三元乙丙橡胶（EPDM）、乙烯一丙烯酸乙酯共聚物(EEA)、相容剂马来酸酐接枝PE、硅烷偶联剂A-171、引发剂DHBP、催化剂二丁基醋酸锡、促进剂DM、活性剂氧化镁、抗氧剂1010、防老剂RD、软化剂邻苯二甲酸二辛酯、润滑剂硬脂酸钙、硅氮阻燃剂、补强剂白炭黑和填充剂陶土放到捏炼机混炼10～12分钟；再将混炼好的材料在温度为40～90℃虑橡机过滤；将过滤后的橡胶材料在辗页机上辗成厚度0.7-2mm的橡胶薄片，经过冷却后制得环保节能自然交联橡胶材料；生产的橡胶材料的拉伸强度为8.7MPa，断裂伸长率为460%。用挤橡机在50～80℃挤出生产矿用电缆、电力电缆、通用橡套电缆、船用电缆等电缆产品。
使用本环保节能自然交联橡胶材料生产矿用电缆时，其材料性能如下：
| 实验内容 | 实施例4 |
| 拉伸强度变化率 | 8.5% |
| 断裂伸长变化率 | 6.7% |
| 载荷下伸长率 | 20% |
| 冷却后永久变形 | 2% |
实施例5和实施例4同样是以生产矿用电缆材料为例， 其它的同实施例4，所不同的是阻燃剂为氢氧化镁，润滑剂为硬脂酸锌。
实施例6和实施例4同样是以生产矿用电缆材料为例， 其它的同实施例4，所不同的是相容剂为马来酸酐接枝EPDM，填充剂为滑石粉。
Claims (1)
1.一种环保节能自然交联橡胶材料的生产方法，其特征在于，所述的橡胶材料是由以下重量份数原料组成：
组成 配比
丁基橡胶IIR 100
乙烯一醋酸乙烯共聚物EVA 15
相容剂为马来酸酐接枝EVA 5
硅烷偶联剂A-172 2
引发剂DCP 0.1
催化剂DBTBL 2
促进剂TETD 1.5
活性剂氧化锌 10
抗氧剂264 1
防老剂MB 1
软化剂石蜡 10
润滑剂硬脂酸 1
氢氧化铝阻燃剂 60
补强剂为半补强炭黑 50
填充剂为碳酸钙 80；
所述的橡胶材料的生产方法是，按上述配比先将丁基橡胶IIR、乙烯一醋酸乙烯共聚物EVA、相容剂马来酸酐接枝EVA、硅烷偶联剂A-172、引发剂DCP、催化剂DBTBL、促进剂TETD、活性剂氧化锌、抗氧剂264、防老剂MB、软化剂石蜡、润滑剂硬脂酸、氢氧化铝阻燃剂、补强剂半补强炭黑和填充剂碳酸钙放到捏炼机混炼10～12分钟；再将混炼好的材料在温度为40～90℃滤 橡机过滤；将过滤后的橡胶材料在辗页机上辗成厚度0.7-2mm的橡胶薄片，经过冷却后制得环保节能自然交联橡胶材料。
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